The appearance of an extrudate formulation was monitored during hot-melt extrusion (HME) continuous manufacturing over 3 days. The formulation matrix consisted of a polymeric component, copovidone, and a low molecular weight surfactant, polysorbate 80. Based on studies prior to the continuous manufacturing, the desired appearance of the target extrudate is translucent. Although process parameters such as feed rate and screw speed were fixed during the continuous manufacturing, the extrudate appearance changed over time from turbid to translucent. For root-cause investigation, the extrudates were analyzed offline by differential scanning calorimetry (DSC) and advanced polymer chromatography (APC™). Although the polysorbate 80 content of both turbid and translucent extrudates was within target, the glass transition temperature of the turbid extrudate was 2 °C above expected value. The observed turbidity was traced to lot-to-lot variability of the polysorbate 80 used in the continuous manufacturing, where APC™ analysis revealed that the relative content of the low molecular weight component varied from 23% to 27% in correlation with the evolution from turbid to translucent extrudates. This work stresses the importance of taking feeding material variability into account during continuous manufacturing.

Synthetic hydrocarbon aviation lubricating oils (SHALOs) gradually degrade over time when subjected to high temperatures, resulting in their composition and properties varying over the operation lifetime. Therefore, understanding the SHALO degradation properties by elucidating the mechanism on a molecular level, as a function of high temperature, is of interest. A SHALO was subjected to thermal treatment (TT) at 180, 200, 230, 250, 270, or 300 °C for 2 h. The chemical compositions of six TT samples and one fresh oil were analyzed by fourier transform infrared F spectroscopy, advanced polymer chromatography, and gas chromatography/mass spectrometry. Furthermore, the physicochemical properties, such as kinematic viscosity, pour point, and acid number, of seven samples were determined. The oil samples were grouped by cluster analysis (CA) using a statistical method. The SHALO was identified to comprise 20 functional groups, including comb-like alkanes, long-chain diesters, amines, phenols, and other compounds. TT at <230 °C caused partial cracking of the SHALO base oils, with a concomitant change in the antioxidant content and type, and the polycondensation reactions were dominant. The observed antioxidant changes were not obvious from TT at >230 °C. A large number of small-molecule compounds were detected, including n-alkanes and olefins. TT at 250 °C was shown to be an important threshold for the kinematic viscosity, pour point, and acid number of the samples. Below 250 °C, the sample properties were relatively stable; but at elevated TT temperatures (>250 °C), the properties were observed to dramatically degrade. As the sample color was highly sensitive to temperature, the TT temperature induced rapid and significant color changes. The CA analysis results for the oil compounds at the molecular level were in good agreement with observed changes in the physicochemical properties at the macro level.

Depolymerized lignin products are very complex mixtures. Based on a depolymerization solution of commercially available sodium lignosulfonate under mild conditions, a fast and efficient method for the separation and direct characterization of the degree and efficiency of the acid-catalyzed depolymerization of lignin was developed in this study. Using an ultraviolet detector, the depolymerized lignosulfonate products were well separated and characterized according to the relative molar mass distribution on an advanced polymer chromatographic system with three ethylene-bridged hybrid columns having small pore sizes (45 Å) in series and tetrahydrofuran as the mobile phase. The developed advanced polymer chromatography method enabled the detection of low-molecular-weight lignin degradation products (Mn  = 260-1100 Da) with high peak resolutions in less than 7.2 min. Furthermore, preliminary advanced polymer chromatography studies to determine the influence of reaction temperature on the depolymerized products indicated that the depolymerized aromatics fell in several molecular weight ranges with an extremely low dispersity. This new approach can be used for the rapid analysis of lignin depolymerization products.

The effects of testing conditions, such as pH and ionic strength of the mobile phase, on the relative molecular mass obtained by advanced polymer chromatography (APC) were investigated systematically. The non-size exclusion effects were discussed for lignosulfonate and its ultrafiltration fractionation product. The relative molecular mass distribution of lignosulfo-nate was well-characterized by an APC system using three columns in series, with a 10 μ L injection volume and 0.1 mol/L NaNO3 as the aqueous mobile phase, at a flow rate of 0.5 mL/min. The relative molecular mass distribution is in the eight molecular mass ranges. Optimized test conditions were used to characterize the ultrafiltration fractionation product of lignosulfonate. The obtained number average relative molecular masses (Mn) of the three components were 40410, 12208, and 1516 Da, indicating that lignosulfonate was well separated into three fractions by ultrafiltration membrane separation. The APC technique presented herein provides the basis for further application of the fractional separation products of lignosulfonate.